Foodstuffs - Determination elements and their chemical species - Determination of aluminium by inductively coupled plasma mass spectrometry (ICP-MS)

This document specifies a method for the determination of aluminium in food by inductively coupled plasma mass spectrometry (ICP-MS) after pressure digestion. This method is suitable for mass fractions in the range of 1 mg/kg to 200 mg/kg. At concentrations above 200 mg/kg digestion temperatures higher than 220 °C can be necessary to recover the aluminium as completely as possible.

Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von Aluminium mit der Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)

Dieses Dokument legt ein Verfahren zur Bestimmung von Aluminium in Lebensmitteln mittels Massen-spektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) nach Druckaufschluss fest. Dieses Verfahren wurde für Säuglingsnahrung, Weizennudeln, Käse, Leber, rote Bete und Kakaopulver mit Massenanteilen im Bereich von 1 mg/kg bis 200 mg/kg validiert. Bei Konzentrationen über 200 mg/kg können höhere Aufschlusstemperaturen als 220 °C notwendig sein, um das Aluminium möglichst vollständig zu erfassen.

Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage de l'aluminium par spectrométrie de masse avec plasma à couplage inductif (ICP-MS)

Le présent document spécifie une méthode de dosage de l’aluminium dans les aliments par spectrométrie de masse avec plasma à couplage inductif (ICP-MS) après digestion sous pression. Cette méthode a été validée pour les préparations pour nourrissons, les nouilles de blé, le fromage, le foie, la betterave et la poudre de cacao, pour des fractions massiques allant de 1 mg/kg à 200 mg/kg. À des fractions massiques supérieures à 200 mg/kg, des températures de digestion dépassant 220 °C peuvent être nécessaires pour obtenir un taux de récupération maximal de l’aluminium.

Živila - Določevanje elementov in njihovih spojin - Določevanje aluminija z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS)

Ta dokument določa metodo za določevanje aluminija v hrani z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS) po razklopu pod tlakom. Ta metoda je primerna za masne deleže v območju od 1 mg/kg do 200 mg/kg. Pri koncentracijah nad 200 mg/kg bodo morda potrebne temperature razklopa nad 220 °C, da se aluminij pridobi v čim bolj popolni obliki.

General Information

Status
Published
Public Enquiry End Date
09-Oct-2018
Publication Date
14-Oct-2019
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
24-Sep-2019
Due Date
29-Nov-2019
Completion Date
15-Oct-2019

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SLOVENSKI STANDARD
SIST EN 17264:2019
01-november-2019

Živila - Določevanje elementov in njihovih spojin - Določevanje aluminija z masno

spektrometrijo z induktivno sklopljeno plazmo (ICP-MS)

Foodstuffs - Determination elements and their chemical species - Determination of

aluminium by inductively coupled plasma mass spectrometry (ICP-MS)
Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Bestimmung von
Aluminium mit der Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS)

Produits alimentaires - Dosage des éléments et de leurs espèces chimiques - Dosage de

l'aluminium par spectrométrie de masse avec plasma à couplage inductif (ICP-MS)
Ta slovenski standard je istoveten z: EN 17264:2019
ICS:
67.050 Splošne preskusne in General methods of tests and
analizne metode za živilske analysis for food products
proizvode
SIST EN 17264:2019 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 17264:2019
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SIST EN 17264:2019
EN 17264
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2019
EUROPÄISCHE NORM
ICS 67.050
English Version
Foodstuffs - Determination of elements and their chemical
species - Determination of aluminium by inductively
coupled plasma mass spectrometry (ICP-MS)

Produits alimentaires - Dosage des éléments et de leurs Lebensmittel - Bestimmung von Elementen und ihren

espèces chimiques - Dosage de l'aluminium par Verbindungen - Bestimmung von Aluminium mittels

spectrométrie de masse avec plasma à couplage Massenspektrometrie mit induktiv gekoppeltem

inductif (ICP-MS) Plasma (ICP-MS)
This European Standard was approved by CEN on 28 July 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17264:2019 E

worldwide for CEN national Members.
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SIST EN 17264:2019
EN 17264:2019 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 3

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 4

5 Reagents ............................................................................................................................................................. 4

6 Apparatus ........................................................................................................................................................... 6

7 Procedure........................................................................................................................................................... 7

7.1 Digestion ............................................................................................................................................................ 7

7.2 Mass spectrometry with inductively coupled plasma ....................................................................... 8

8 Evaluation ....................................................................................................................................................... 10

8.1 Calculation ...................................................................................................................................................... 10

8.2 Precision .......................................................................................................................................................... 10

8.3 Repeatability .................................................................................................................................................. 10

8.4 Reproducibility ............................................................................................................................................. 11

9 Test report ...................................................................................................................................................... 11

Annex A (informative) Results of interlaboratory study ............................................................................ 12

Annex B (normative) Explanation notes ........................................................................................................... 14

Bibliography ................................................................................................................................................................. 16

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SIST EN 17264:2019
EN 17264:2019 (E)
European foreword

This document (EN 17264:2019) has been prepared by Technical Committee CEN/TC 275 “Food

analysis - Horizontal methods”, the secretariat of which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by March 2020, and conflicting national standards shall

be withdrawn at the latest by March 2020.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
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SIST EN 17264:2019
EN 17264:2019 (E)
1 Scope

This document specifies a method for the determination of aluminium in food by inductively coupled

plasma mass spectrometry (ICP-MS) after pressure digestion. This method was validated for infant

formula, wheat noodle, cheese, liver, beetroot and cocoa powder at mass fractions in the range of

1 mg/kg to 200 mg/kg. At concentrations above 200 mg/kg, digestion temperatures higher than 220 °C

can be necessary to recover the aluminium as completely as possible.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

EN 13804, Foodstuffs - Determination of elements and their chemical species - General considerations and

specific requirements
EN 13805, Foodstuffs - Determination of trace elements - Pressure digestion

EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)

3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle

Aluminium is determined quantitatively by ICP-MS after digestion of the sample with nitric acid (with

addition of water in case of foods with low water content) according to the pressure digestion process

described in EN 13805 but without the use of hydrofluoric acid. The digestion conditions are chosen in

such a way that even for samples with aluminium compounds of low solubility (e.g. silicates, oxides)

low findings are kept to a minimum.
5 Reagents

The mass concentration of aluminium shall be low enough in the reagents and water not to affect the

results.

All reagents shall be of analytical grade, i.e. pro analysi, p.a. or similar unless otherwise specified.

Use water conforming to grade 2 of EN ISO 3696.
5.1 Nitric acid, mass fraction w = at least 65 %, density = 1,4 g/ml.

5.2 Aluminium stock solution, with a certified mass concentration ρ = 1 000 mg/l.

5.3 Rhodium stock solution, ρ = 1 000 mg/l as internal standard.

The internal standard shall be free from aluminium impurities and shall be present in the sample in

negligibly small amounts only.
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SIST EN 17264:2019
EN 17264:2019 (E)

Rhodium and Indium are suitable as internal standards. Other internal standards, especially those

having mass/charge ratios (m/z) < 100, shall not be used, since molecule ion interferences can distort

the measurement.

NOTE The verification of molecule ion interferences was performed in the collaborative study using a high-

resolution ICP mass spectrometer with a resolution of R = 4 000 .
5.4 Standard solutions
5.4.1 General

When preparing solutions special care shall be taken to avoid contaminations. For aluminium there are

various sources of contamination, e.g. volumetric flasks made of glass. Annex B of this document

requires special attention.
5.4.2 Aluminium standard solution 1, ρ = 10 mg/l.

Fill 10 ml of water into a 50-ml volumetric flask; add 2 ml of nitric acid (5.1) and mix. After cooling

down to room temperature, pipette exactly 500 µl of the aluminium stock solution (5.2) to the flask, and

fill up with water to the mark. This standard solution 1 is stable for at least 3 months.

5.4.3 Aluminium standard solution 2, ρ = 1 mg/l.

Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.

After cooling down to room temperature, pipette exactly 5 ml of the aluminium standard solution 1 of

ρ = 10 mg/l (5.4.2) to the flask and fill up with water to the mark. This standard solution 2 is stable for

at least 3 months.
5.4.4 Aluminium standard solution 3, ρ = 0,1 mg/l.

Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.

After cooling down to room temperature, pipette exactly 5 ml of the aluminium standard solution 2 of

ρ = 1 mg/l (5.4.3) and fill up with water to the mark. This standard solution 3 is stable for at least

3 months.
5.4.5 Rhodium standard solution 1 (internal standard solution 1), ρ = 10 mg/l.

Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.

After cooling down to room temperature, pipette exactly 500 µl of the rhodium stock solution (5.3) to

the flask and fill up with water to the mark. This internal standard solution 1 is stable for at least

3 months.
5.4.6 Rhodium standard solution 2 (internal standard solution 2), ρ = 1,0 mg/l.

Fill approximately 10 ml of water into a 50-ml volumetric flask, add 2 ml of nitric acid (5.1) and mix.

After cooling down to room temperature, pipette exactly 5 ml of the rhodium standard solution 1 of

ρ = 10 mg/l (5.4.5) and fill up with water to the mark. This internal standard solution 2 is stable for at

least 3 months.
1) resolution R = m/Δm.
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SIST EN 17264:2019
EN 17264:2019 (E)
5.5 Aluminium calibration solutions

The mass concentrations of the calibration solutions described are examples and may be changed

according to the sensitivity of the measuring instrument and the concentration range to be analysed.

Make sure that the calibration is carried out within the linear range of the detector system. For

calibration, at least 3 calibration solutions of different concentrations should be prepared. Make sure

that the acid concentration of the calibration solutions corresponds to the test solution.

In order to avoid contaminations originating from the flask material, do not use volumetric flasks made

from borosilicate glass. Note the information on contaminations provided in B.1.

Prepare the calibration solutions from aluminium standard solution 2 and 3 (5.4.3 and 5.4.4) according

to the following scheme in Table 1:
Table 1 — Example of aluminium calibration solutions
Calibration Volume of aluminium Volume of internal Mass concentration of
solution no standard solution standard solution 2 aluminium in the
(5.4.6) calibration solution
µl µg/l
1 200 µl of standard solution 3 200 1
(5.4.4)
2 100 µl of standard solution 2 200 5
(5.4.3)
3 500 µl of standard solution 2 200 25
(5.4.3)
4 2000 µl of standard solution 2 200 100
(5.4.3)

EXAMPLE Fill 4 ml to 5 ml of water into a 20 ml volumetric flask, add 250 µl of nitric acid (5.1), and mix.

After cooling down to room temperature, pipette the standard solution and the internal standard solution 2

according to Table 1 to the flask, fill up to the mark with water and mix.

Alternatively, the internal standard can be pumped into the sample flow via a Y-piece during

measurement. In this case, the internal standard solution is not pipetted into the calibration solutions.

NOTE The acid concentration of the calibration solution in the example is adapted to a digestion with 2,5 ml

of nitric acid (5.1), a filling volume of 20 ml and a dilution factor of 10 (in case of a dilution with water).

The calibration solutions shall be freshly prepared each working day.
5.6 Zero-point solution

For the zero-point solution, add 1,25 ml of nitric acid (5.1) and if applicable the internal standard 2 (in

exactly the same mass concentration as in the calibration solutions, according to the example given

in 5.5) to a 100 ml volumetric flask and fill up with water.
6 Apparatus

All equipment and labware that come into direct contact with the sample and the solutions used shall

be carefully pretreated/cleaned according to EN 13804 to minimize the blank value (see Annex B for

details). In addition to standard laboratory equipment, use the following:
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SIST EN 17264:2019
EN 17264:2019 (E)
6.1 Inductively coupled plasma mass spectrometer (ICP-MS).

The ICP-MS shall include inductively coupled argon plasma, sample supply and nebulising system as

well as instrument controlling and data acquisition. In order to avoid interferences on the atomic mass

of aluminium, it can be necessary to use a mass spectrometer that is able to delete or minimize

interferences (e.g. which is equipped with cell technology or resolution above 300) [1].

6.2 Digestion vessels, e.g. of polyfluoropolymers or quartz with volumes from 70 ml to 100 ml.

6.3 Test tube shaker, optional.
6.4 Analytical balance, capable to weigh to the nearest milligram.
7 Procedure
7.1 Digestion
7.1.1 General
To ensure complete dissolution of aluminium the following shall be respected:
— ensure that the sample is sufficiently homogeneous;

— in case of incomplete digestion or high aluminium contents, it may be beneficial to use a test

portion as small as possible (at least 200 mg for dry samples) in order to digest aluminium

compounds as completely as possible;

— for samples containing silicates, digestion temperatures above 220 °C may be necessary in order to

dissolve the aluminium as completely as possible;

— in case of samples with low water content, first add water and mix intensively, before adding

concentrated nitric acid;
— do not use hydrogen peroxide for digestion.

Further information regarding test portions and digestion are given in B.2 and B.3.

For pressure digestion according to EN 13805, different vessels may be used depending on the

instrument type and manufacturer. The maximum test portion and the minimum liquid volume depend

on the pressure stability of the respective vessels. The specifications according to 7.1.2 refer to

digestion vessels with volumes from 70 ml to 100 ml and a minimum liquid volume of 5 ml.

All indications in 7.1.2 shall be adjusted to the digestion instrument used. For safety reasons the

manufacturer's specifications shall be strictly followed.
7.1.2 Digestion procedure

Before digestion, different amounts of water, depending on the different types of food [2], are added in

order to obtain comparable acid concentrations in the final digestion solution. The amount of water to

be added depends on the test portion and thus on the content of carbon and water in the food type.

Add just as much water to the initial test portion that is necessary to suspend the food completely. Then

complete the test portion with water to reach 3 g. Water is also added to fat-containing foods, even if a

suspension is hardly possible.
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SIST EN 17264:2019
EN 17264:2019 (E)

Example for digestion of powdery food: Add 2,5 ml of water to the dry food, e.g. 0,5 g of flour. Mix the

contents of the digestion vessel intensively, e.g. on a test-tube shaker. Repeat shaking every 10 min to

15 min until the susp
...

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